• 제목/요약/키워드: Reversed-phase HPLC

검색결과 357건 처리시간 0.023초

역상 HPLC에 의한 홍국 중의 락톤 및 산성 모나콜린 K의 동시분석법 (Simultaneous Analysis of Both Lactone Form and Acid Form Monacolin K in Red Yeast Rice by RP-HPLC)

  • Moon, Young-ja;Wang, Qi-jun;Xu, Bao-jun;Li, Chang-tian;Kim, Jae-hoon;Mo, En-kyeng;Baek, Seoung-young;Il Kwon;Sung, Chang-keun
    • 한국식품영양학회지
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    • 제14권6호
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    • pp.521-526
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    • 2001
  • 홍버섯쌀은 현재 혈압과 혈중 고지혈 강하제로서 의약품 뿐만 아니라 기능성 식품으로서 많은 관심을 불러일으키고 있다. 그러나 이 홍버섯에 함유된 유효성분인 monacolin K의 정성법과 정량적인 분석 방법이 제시되지 못하였다. 본 연구에서는 monacolin K의 lactone과 acid 형태에 대한 각각의 정확한 정성법과 정량가능한 분석법을 제안하였다. 이 방법은 HPLC의 역상컬럼을 사용하여 acetonitrile과 0.1%TFA를 62:38의 비율로 혼합한 용매를 사용하는 것이다. 이 제시된 방법을 활용했을 때 홍국중의 monacolin K의 최소 검출농도는 5ng이었다.

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역상 액체 크로마토그래피에 의한 금속-2-hydroxyarylazopyrazolone 유도체 킬레이트의 용리거동 및 동시분리에 관한 연구 (I) (Separation and Elution Behaviors of Some Metal-2-hydroxyarylazopyrazolone Chelates by Reversed Phase High Performance Liquid Chromatography (I))

  • 이창헌;강창희;김은경;이원
    • 분석과학
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    • 제7권1호
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    • pp.103-114
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    • 1994
  • 네 가지 2-hydroxyarylazopyrazolone 유도체를 합성하고, 이를 리간드로 사용하여 Ni(II), Cu(II), Co(III), Cr(III)의 금속이온들과 2-hydroxyarylazopyrazolone의 킬레이트를 합성하였다. 합성한 pyrazolone 유도체 및 금속 킬레이트의 구조는 IR, MS, UV-Visible, ICP 등의 분광법으로 확인하였다. 역상 액체 크로마토그래피에서 이들 금속 킬레이트 화합물들에 대한 동시 분리의 가능성 및 머무름 메카니즘을 확인하기 위하여 분리관의 종류, 용리액의 조성, 흐름 속도 등 최적 분리조건을 조사한 결과 Novapak $C_{18}$ 분리관과 용리액으로 사용한 메탄올과 물의 혼합비율을 적절히 조절했을 때 용량인자(k')는 $0{\leq}log\;k^{\prime}{\leq}1$의 범위를 만족시켰다. 또한 용량인자와 용리액 중 물의 부피분율 및 분포계수($D_c$)와의 상관 관계들을 조사한 결과 이들의 상호 직선적인 비례관계를 나타내었고, 이로부터 분리관 내에서 이들 금속 킬레이트의 용리거동이 소용매성 효과에 기인하고 있음을 확인하였다.

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HPLC를 이용한 우유중의 클로람페니콜의 정량 분석 (Determination of Chloramphenicol in Milk by High Performance Liquid Chromatography)

  • 김경례;김정한;최경숙
    • 약학회지
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    • 제29권1호
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    • pp.50-54
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    • 1985
  • Seven different sorbents were evaluated for their adsorptivity and desorptivity of antibiotic, chloramphenicol. Among the sorbents studied, Carbopak B was found to be the most efficient in enriching the chloramphenicol from dilute aqueous solution. Interfering components in the milk matrix could be washed off by water and petroleum ether from Carbopak B column, while the chloramphenicol was retained on the surface of Carbopak B. The method of simple and efficient purification and enrichment of chloramphenicol using Carbopak B, followed by quantitative analysis employing $C_{18}$ reversed phase high performance liquid chromatography has been applied to the determination of chloramphenicol in milk.

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Reversed-phase 및 $Ag^{+}$-HPLC에 의한 Conjugate Trienoic Acid 함유(含有) Triacylglycerol 분자종(分子種)의 상호분리(相互分離) (Resolution of the Triacylglycerols Containing Conjugate Trienoic Acids into Their Molecular Species by HPLC in the Reversed-phase and Silver Ion Mode)

  • 김성진;우효정;조용계
    • 한국응용과학기술학회지
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    • 제18권3호
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    • pp.197-213
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    • 2001
  • Conjugate trienoic acids (CTA) occurred in triacylglycerols (TGs) of the seed oils of Trichosanthes kirilowii, Momordica charantia and Aleurites fordii, and they were easily converted to their methyl esters in a mixture of sodium methoxide-methanol without any structural destruction. The main fatty acids in triacylglycerol (TG) fraction of the seed oils of Trichosanthes kirilowii are $C_{18:2{\omega}6}$ (32.2 mol %), $C_{18:3{\;}9c.11t,13c}$ (38.0 mol %) and $C_{18:1{\omega}9}$ (11.8 mol %), followed with $C_{16:0}$ (4.8 mol %) and $C_{18:0}$ (3.1 mol %). The TG fraction was resolved into 20 TG molecular species according to the partition number (PN) by reversed-phase (RP)-HPLC. The main TG species were $DT_{c2}$, $MDT_{c}$ and $D_{2}T_{c}$, of which amounts reached 63 mol % of total TG molecular species. The TG sample was fractionated into 11 fractions according to the number of double bond in the molecule by $Ag^{+}-HPLC$ and the species of $DT_{c2}$, $MDT_{c}$ and $D_{2}T_{c}$ were also eluted as main components. The TG species containing CTA showed unusual behaviours in the order of elution by HPLC ; first, TG moleular species of $DT_{c2}$ (D; dienoic acid, $T_{c}$; punicic acid, $T_{ci}$; ${\alpha}-eleostearic$ acid, M ; monoenoic acid, $S_{t}$; stearic acid) was eluted earlier than $Mt_{c2}$, although they have the same PN number of 40, and, secondly, the species of $DT_{ci2}$ with eight double bonds was eluted earlier than that of $D_2T_{ci}$ with seven double bonds. Intact TG of the seed oils of Momordica charantia contained mainly fatty acids such as $C_{18:3{\omega}9c,11t,13t}$ (57.7 mol %), $C_{18:1{\omega}9}$ (17.4 mol %), $C_{18:0}$ (12.3 mol %) and $C_{18:2{\omega}6}$ (10.6 mol %), and was classified into 13 fractions by RP-HPLC. The main TG species were as follows ; $MT_{ci2}$ [$(C_{18:1{\omega}9})(C_{18:3\;9c,11t,13t})_{2}$, 39.1 mol %] and $S_{t}T_{ci2}$ [$(C_{18:0})(C_{18:3\;9c,11t,13t})_2$, 33.9 mol %] comprising about 73 mol % of total TG species, accompanied by $DT_{ci2}$ [$(C_{18:2{\omega}6})(C_{18:3\;9c,11t,13t})_{2}$, 7.3 mol %], $D_{2}T_{ci}$ [$ (C_{18:2{\omega}6})_{2}(C_{18:3\;9c,11t,13t})$, 3.6 mol %] and $MDT_{ci}$ [$(C_{18:1{\omega}9})(C_{18:2{\omega}6})(C_{18:3\;9c,11t,13t})$, 3.5 mol %]. Simple TG species of $T_{ci3}$ [$(C_{18:3\;9c,11t,13t})_3]$ was present in a small amount of 1.4 mol %, but other simple TG species were not detected. The TG was also resolved into 11 fractions according to the number of double bond by $Ag^{+}-HPLC$, and the species were mainly occupied by $MT_{ci2}$ [$(C_{18:1{\omega}9})(C_{18:3\;9c,11t,13t})_{2}$, 39.4 mol %] and $S_tT-{ci2}$ [$(C_{18:0})(C_{18:3\;9c,11t,13t})_{2}$, 35.4 mol %] $DT_{ci2}$ species with eight double bonds was also developed faster than $D_2T_{ci}$ one with seven double bonds as indicated in the analysis of TG of the seed oils of T. kirilowii, and $MT_{ci2}$ species with cis, trans, trans-configurated double bond was eluted earlier than $MT_{c2}$ species with cis, trans, cis-configurated double bond. The main components of fatty acid in total TG fraction isolated from the seed oils of of Aleurites fordii were in the following order ; $C_{18:3\;9c,11t,13t}$ (81.2 mol %)> $C_{18:2{\omega}6}$ (8.5 mol %)> $C_{18:1{\omega}9}$ (5.4 mol %)$. With resolution of the TG by RP-HPLC, eight fractions such as $T_{ci3}$, $Dt_{ci2}$, $D_{2}T_{ci}$, $MT_{ci2}$, $PT_{ci2}$ (P; palmitic acid), $PMT_{ci}$, $PDT_{ci}$ and $S_{t}T_{ci2}$ ($S_{t}$; stearic acid) were isolated, respectively. TG species of $T_{ci3}$ [$(C_{18:3\;9c,11t,13t})_{3}$, 54.2 mol %], $DT_{ci2}$ [$(C_{18:2{\omega}6})(C_{18:3\;9c,11t,13t})_{2}$, 15.0 mol %] and $MT_{ci2}$ [$(C_{18:1{\omega}9})(C_{18:3 9c,11t,13t})_{2}$, 14.8 mol %] were present as main species.

HPLC Separation of Isoquinoline Alkaloids for Quality Control of Corydalis species

  • Kim, Eun-Kyung;Jeong, Eun-Kyung;Han, Sang-Beom;Jung, Jee-H.;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • 제32권10호
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    • pp.3597-3602
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    • 2011
  • A simple and rapid analytical method was developed for the determination of eight isoquinoline alkaloids in Corydalis species. Eight isoquinoline alkaloids, including 2 aporphine alkaloids (isocorydine and glaucine) and 6 protoberberine alkaloids (coptisine, palmatine, berberine, canadine, corydaline, and tetrahydrocoptisine) were used as chemical markers which have a various biological activity and determined for quality control of Corydalis (C.) species (C. ternata, C. yanhusuo, and C. decumbens). To evaluate the quality of these herbal medicines, LC chromatographic separation of alkaloids were preferentially investigated on reversed-phase C18 column with pH variation and composition of mobile phase. In addition, the separation of these alkaloids in herbal extracts was found to be significantly affected on mobile phase composition using gradient elution. Especially for C. yanhusuo extract, berberine was seriously interfered with other alkaloid extracted from sample matrix when mobile phase composition was not optimized. As results, these compounds were successfully separated within 28 min using 10 mM ammonium acetate containing 0.2% triethylamine (adjusted at pH 5.0) as a mobile phase with gradient elution. On the basis of optimized HPLC conditions, 23 different Corydalis species samples were analyzed for the determination of alkaloid levels. In addition, principal component analysis (PCA) combined with the chromatographic data could be successfully classified the different geographic origin samples.

녹차에서 카테킨 화합물의 초임계 유제 추출 (Supercritical Fluid Extraction of Catecnin Compounds from Green Tea)

  • 나영진;이윤우;김재덕;노경호
    • KSBB Journal
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    • 제16권4호
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    • pp.327-331
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    • 2001
  • 전라남도 보성산 녹차로부터 유용성분인 카테킨 화합물을 초임계 이산화 탄소와 첨가제를 사용하여 추출하고 역상 고성능 액체 크로마토그래피(RP-HPLC)를 사용하여 분석하였다. LiChrospher 100RP-18(15 $\mu$m)로 충진된 column을 이용하여 0.05% phosphoric acid가 포함된 물과 acetonitrile을 이동상으로 사용하였으며 구배용매 조성법을 적용하였다. 이동상의 조성에 따른 체류인자의 조절을 통해 EGCG를 분리하였다. 각각의 초임계 추출법에 따른 EGCG의 추출량을 비교한 결과, 초임계 유체에 극성물질을 포함하는 경우가 녹차의 유용 성분인 EGCG의 추출량이 가장 많았다. 그러나 ethanol에 의한 용매 추출법은 초임계 유체에 의한 추출법보다 EGCG에 대해 많은 추출양과 선택적인 고순도 분리가 가능하였다.

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Impurity Profiling and Quantification of Sudan III Dyes by HPLC-selective UV Detection

  • Yang, Ki Ryeol;Hong, Ji Yeon;Yoon, Soo Hwan;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • 제35권3호
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    • pp.765-769
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    • 2014
  • An analytical methodology was developed for qualitative and quantitative impurity profiling of the coloring agent Sudan III by high-performance liquid chromatography (HPLC)-diode array detection (DAD). The impurities in commercial Sudan III were characterized by comparison of their retention times and UV spectra with those of authentic standards. Four impurities regulated by International Committees in Sudan III were quantified by HPLC-selective UV detection. The impurities in Sudan dye were successfully separated on a reversed phase C18-column within 25 min and sensitively detected by UV spectrometry at two selective wavelengths. Method validation was conducted to determine linearity, precision, accuracy, and limit of quantification (LOQ). The linear dynamic range extended from 0.002 to 4.0%, with a correlation coefficient (R2) greater than 0.995. The LOQs of the impurities ranged from 8.04 to $54.29{\mu}g/mg$. Based on the established method, the levels of regulated impurities in five commercial Sudan III dyes were determined.

HPLC를 이용한 목향 및 유사 한약재에 함유된 Costunolide 비교 (Determination of Costunolide from Aucklandiae Radix and Substitutive Herbs by Reversed-Phase HPLC)

  • 오주희;홍선표;최호영;박용기;이제현
    • 대한본초학회지
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    • 제23권3호
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    • pp.61-66
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    • 2008
  • Objecives : Aucklandiae Radix is a root of Aucklandia lappa which has been widely used for regulating the flow of vital energy, invigorating the spleen, alleviating pain. Aucklandiae Radix contains the costunolide which is the main ingredient. The substitutive Aucklandiae Radix are Inulae helenii Radix, Aristolchiae Radix, Vladimiriae Radix, and Inulae racemosi Radix in Korea and China. This paper is analysised and compared the costunolide and HPLC pattern in Aucklandiae Radix and substitute herbs. Methods : Chromatographic separation performed using C18 column(Luna 5 u, 250 mm ${\times}$ 4.6 mm) with a mixture of methanol and water(65:35)(v/v). The analyses detected at UV(210 nm). Results : Optimal extraction condition of costunolide was 100% methanol for 2hr. Costunolide was detected in Aucklandiae Radix and Vladimiriae Radix, but other herbs were not detected. In Korea herbal market, Aristolchiae Radix merchandise was identified as the imported Inulae helenii Radix. Conclusions : According to above results, this method was useful identified to Aucklandiae Radix and substitutive herbs. In Korea herbal market, Aristolchiae Radix was identified as Inulae helenii Radix.

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Identification of IY81149 and Its Metabolites in the Rat Plasma Using the On-Line HPLC/ESI Mass Spectrometry

  • Myung, Seung-Woon;Min, Hye-Ki;Jin, Chang-Bae;Kim, Myung-Soo;Lee, Seung-Mok;Chung, Gi-Ju;Park, Seong-Jun;Kim, Dong-Yeon;Cho, Hyun-Woo
    • Archives of Pharmacal Research
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    • 제22권2호
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    • pp.189-193
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    • 1999
  • Reversed-phase high-performance liquid chromatography/mass spectrometry (HPLC/MS) with an eletcrospray ionization (ESI) interface was applied to the identification of metabolites of IY81149 in the rat plasma. Fragments obtained using collision-induced dissociation (CID) in both positive and negative modes were utilized to elucidate the structure of metabolites. The eluent from the conventional HPLC column was split and directly introduced into an ESI-mass spectrometer for the identification of the structures. the CID technique allowed the sensitive identification of sulfonyl-IY81149 and hydroxy-IY81149 from the rat plasma.

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